CN108516684A - A kind of inorganic adhesive glaze and preparation method thereof - Google Patents

A kind of inorganic adhesive glaze and preparation method thereof Download PDF

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Publication number
CN108516684A
CN108516684A CN201810427597.6A CN201810427597A CN108516684A CN 108516684 A CN108516684 A CN 108516684A CN 201810427597 A CN201810427597 A CN 201810427597A CN 108516684 A CN108516684 A CN 108516684A
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glaze
inorganic adhesive
preparation
parts
parent
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CN108516684B (en
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李玉平
马天齐
郭爱芬
高应霞
肖万芬
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Suzhou Porcelain Insulator Works Co ltd
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Hunan University
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02Frit compositions, i.e. in a powdered or comminuted form
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C03C8/20Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions containing titanium compounds; containing zirconium compounds
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/003Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Glass Compositions (AREA)

Abstract

The present invention relates to a kind of inorganic adhesive glaze and preparation method thereof, and parent glaze, borax and albite are mixed, and parent glaze melt is fired within the scope of 1200 DEG C~1500 DEG C, and water quenching obtains parent glaze frit, spare;Wherein, the additive amount of borax is 2wt%~6wt% of basic glaze, and the additive amount of albite is 2wt%~8wt% of basic glaze;Step S1 is obtained into parent glaze frit and Nucleating Agent mixes, grinding obtains inorganic adhesive glaze.The preparation method thinking of the present invention is novel, and prepared inorganic adhesive glaze adhesive strength is high and stability is strong.

Description

A kind of inorganic adhesive glaze and preparation method thereof
Technical field
The present invention relates to a kind of inorganic adhesive glaze and preparation method thereof, more particularly to one kind are hollow for being bonded extra-high voltage Inorganic adhesive glaze of porcelain insulator and preparation method thereof.
Background technology
With the continuous improvement of project of transmitting and converting electricity voltage class, the height of matched hollow insulator also increases therewith Greatly, as the switch of 800kV porcelain insulator product height reaches 10m or more, 1100 mm have been reached at largest outside diameter.It is this kind of super Large-scale porcelain insulator under prior art conditions, can't using global formation, be integrally burnt by the way of manufacture.Generally all Sectional forming, segmentation firing are taken, is finally again composed the porcelain piece sintered bonding.Organic bonding method and inorganic adhesive method It is common two major classes adhering method.
Organic bonding is bonded porcelain insulator component using resin.Common organic adhesive is mostly epoxy resin, phenol Urea formaldehyde class.The former is mainly formulated by epoxy resin base-material, accelerating agent, curing agent, filler and diluent etc..Because of its bonding Property, it is functional preferably, technique is simpler, cheap, and is widely used.Now to the research and development of epoxy resin also not Disconnected to go deep into, its own performance is constantly improving;The latter is then the resin formed under the action of catalyst by phenols and aldehydes It is referred to as, has many advantages, such as that water resistance, weatherability, temperature tolerance and adhesive strength are high.With deepening continuously for R&D work, phenolic aldehyde Toughness, durability and the electric property of resin are still being continued to optimize.But organic bonding still has deficiency:Easy to aging, brittleness It is still unable to reach ideal value with elasticity, electrical resistance also is difficult to ensure.Therefore, the manufacture of large-scale insulator mostly uses inorganic viscous Connection.Organic bonding is easy to operate, technology maturation.
Inorganic adhesive:I.e. with glaze come bonded ceramics component.Inorganic adhesive glaze and porcelain piece chemical property are stablized, and have excellent Temperature tolerance, oil resistivity, preferable ageing-resistant performance and cost are relatively low, economic and environment-friendly, not will produce problem of aging, product machine generally Tool intensity will not reduce over time with electric property.Inorganic adhesive glaze, after twice firing, glaze melt can ooze Thoroughly in upper lower ceramic part, stronger anastomosis is formd.The large-scale porcelain insulator being bonded with this method has high mechanical strength, Geometric tolerance is smaller, and especially anti-aging property preferably enjoys great popularity.
Realize inorganic adhesive, key is at 2 points, first, designing inorganic adhesive glaze, it is desirable that it must have good electrical Performance, mechanical performance, cold and hot performance and glaze fit etc., what is be even more important it is also desirable to have good adhesive property.Second is that Retrofit must be carried out to bonding site, to make upper and lower two energy saving tight connectings of bonding plane, and can be good at accommodating viscous Glaze is connect, on the bonding plane that the glaze melt for being allowed to be formed at high temperature can be sprawled equably.Glazing area is the space of relative closure. In this case, adhesive glaze generate bubble may be because of being difficult to emit and affect the quality of bonding.
Inorganic adhesive glaze is prepared, has some and did related work.For example, CN1075943A, CN101439988A, CN102757258A etc. discloses the preparation method of some inorganic adhesive glaze.Zhang Xitang(2005)It is inorganic to discuss giant porcelain shell Bonding forming critical process, it is believed that in bonding process, the making of blank, the grinding for filling burning and bonding plane etc. are all to being bonded qualification rate It has a major impact.In above-mentioned several disclosed patents, inorganic adhesive is all carried out using raw glaze.Somebody takes glaze Middle pigment is detached with base glaze, then pre-synthesis colorant, and the pigment of synthesis is then treated as a kind of glaze raw material again, it is added Inorganic adhesive glaze is made in its parent glaze raw material, together grinding.The it is proposeds such as palace rosy clouds, Yang Hai, Yu Yanxia (2013) pass through The generation of gas phase amount in glaze is reduced to improve adhesive strength, they also emphasize will select burnt clinker as far as possible, such as ripe big With raw materials such as, ripe talcums, to reduce the discharge of sintering process volatile matter, but they simultaneously but used dolomite (CaMg (CO3)2) such raw material that can generate bulk gas;They also add ZrO during enamel frit makeing2Micro mist is to can improve glaze Intensity;Although some are improved, from the point of view of existing document, most of inorganic adhesive glaze still fall within the scope of raw glaze, burn At still will produce bubble in the process.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of adhesive strength high and stable inorganic adhesive glaze and its preparation Method.
In order to solve the above-mentioned technical problem, technical scheme is as follows:A kind of preparation method of inorganic adhesive glaze, packet Include following steps:
S1, parent glaze, borax and albite are mixed, is fired into parent glaze melt within the scope of 1200 DEG C~1500 DEG C, water quenching, Parent glaze frit is obtained, it is spare;
Wherein, the additive amount of borax is 2wt%~6wt% of basic glaze, and the additive amount of albite is 2wt%~8wt% of basic glaze;
S2, step S1 is obtained to parent glaze frit and Nucleating Agent mixing, grinding obtains inorganic adhesive glaze;
Wherein, the additive amount of the Nucleating Agent is 1wt%~5wt% of basic glaze frit.
The adhesive glaze of the present invention is added to some functional components, the parent glaze of making based on ripe glaze for electric porcelain Based on frit.Parent glaze frit is combined with Nucleating Agent, is ground so that it becomes a kind of completely new inorganic bond glaze.First will Parent glaze frit is made in parent glaze, and the volatility in branch glaze removal can effectively avoid adhesive glaze and generate hardly possible in follow-up sintering procedure With the bubble of exclusion so that bonding portion is closely knit reliable, promotes adhesive strength;And the addition of Nucleating Agent can make inorganic adhesive glaze Under the high temperature conditions(After bonding in sintering procedure)Part crystallite is formed, the intensity of glaze glass can be improved, it is strong to improve bonding Degree.
Borax and albite mainly play reduction high temperature viscosity, and glass is easy fusing, and can also slightly increased glass expansion Coefficient.
Further, in step S2, step S1 is obtained into parent glaze frit, Nucleating Agent and coloring material for mixing, grinding obtains nothing Machine adhesive glaze
Further, the preparation method of the colorant is:First basic toner, magnesia and borax are mixed, then 900 ~ 1350 1 ~ 3h is kept the temperature under the conditions of DEG C, is then cooled down, is ground, and successively after pickling, cleaning, drying obtains colorant;
Wherein, the additive amount of magnesia is 1 ~ 8wt% of basic toner, and the additive amount of borax is 1 ~ 10wt% of basic toner.
Further, in step S1, firing temperature is 1400-1550 DEG C.
Further, basic toner may be commercially available colorant.
Further, the basic toner includes di-iron trioxide, chrome green, manganese dioxide, is a kind of bronzing agent, The specific proportioning of toner can be selected according to actual needs.
Further, the parent glaze is glaze for electric porcelain, and matching for parent glaze can directly be determined according to the formula of glaze for electric porcelain, tool Body, the pigmentation element for directly removing former glaze for electric porcelain can be used or be in former provide of other raw materials replacement of low pigmentation element content The method of color element raw material designs the electroceramics basis glaze formula without pigmentation element;Common former glaze for electric porcelain can also be used directly to make For the parent glaze of the present invention.
Further, in parts by mass, the parent glaze includes 10-18 parts of feldspar powder, 20-30 parts of silica flour, field master worker Soil or mud 2-6 parts of Hubei, 8-15 parts of porcelain powder, 2-8 parts of calcite, 1-3 parts of talcum powder, 0-3 parts of barium carbonate, 0-2 parts of spodumene.
The Nucleating Agent includes zinc oxide, zirconium silicate, fluorite, kaolinic at least one.
A kind of inorganic adhesive glaze, is made of preparation method as described above.
It, can be first by hollow porcelain insulator to be bonded when inorganic adhesive glaze using the present invention is bonded multiple hollow porcelain insulators Two end surface grindings be processed into the groove being mutually matched and convex surface, wherein positioned at lower part insulator wait for bonding plane be upward opening " V " font groove, and wait for that bonding plane is the pinnacle convex surface directed downwardly in " Λ " font positioned at top porcelain insulator;It will process again Lower part first segment porcelain insulator be located in " top-hat kiln " bottom plate for removing kiln body, by the inorganic adhesive powdered frit refined or Adhesive glaze cream is encased in " V " font groove of lower hollow porcelain insulator, and powdered frit or glaze cream should at least be added in " V " font groove 2/3 or more of depth;The top porcelain insulator that will be bonded again is lifted on first segment porcelain insulator, its " Λ " font is convex Face is precisely positioned in " V " font groove;Top hollow porcelain insulator is gently rotated, makes two section hollow porcelain insulators in coaxial Shape is upright, and makes to wait for that powdered frit or the glaze cream on bonding plane are uniformly distributed, firing, you can(Referring to Fig. 2 and Fig. 3).
The preparation method thinking of the present invention is novel, and prepared inorganic adhesive glaze adhesive strength is high and stability is strong.
Description of the drawings
Fig. 1 is the SEM figures at bonding interface when the inorganic adhesive glaze in embodiment 1 is used to be bonded, wherein(a)1000 times Enlarged drawing,(b)10000 times of enlarged drawings,(c)600 times of enlarged drawings,(d)2000 times of enlarged drawings.
Fig. 2 is that the dress for the test specimen that inorganic adhesive glaze using the present invention is bonded burns photo.
Fig. 3 is the shape photo for the test specimen that the inorganic adhesive glaze of the present invention is bonded.
Specific implementation mode
Below with reference to coming in conjunction with the embodiments, the present invention will be described in detail.
Embodiment 1
A kind of preparation method of inorganic adhesive glaze, includes the following steps:
The present embodiment is that basic glaze analyzes the composition characteristics of glaze for electric porcelain first with glaze for electric porcelain.Glaze for electric porcelain will have good workability Can, such as good suspension and adequately uniformly dispersed can be adsorbed successfully when such glazing by dry body and be formed uniform Glaze layer, can be successfully ripe when high temperature, and forms firm glaze-body bonding layer, can also improve the mechanical strength of electroceramics in addition.
For example, the brown glaze of certain electroceramics manufacturing company, 5# palm fibres glaze formula therein is especially ripe, on its basis, carries out Slight adjustment forms 6#, 7# formula(It is shown in Table 1).Its primary raw material has feldspar powder, quartz sand, field soil, base mud, field master worker, porcelain Powder, calcite, talcum powder and iron, chromium, the oxide of manganese, barium carbonate etc..Iron oxide in brown glaze is from field soil, and 7# formulas are also Add a small amount of iron oxide.
1 three kinds of electroceramics palm fibre glaze proportionings (wt%) of table
When dispensing, precise above-mentioned raw materials, for 24 hours with ball mill grinding, 3 glaze slurries are respectively in tailing over of sieving of 320 mesh 0.037%、0.025%、0.031%.It applies in electroceramics strip, glazed thickness is about 0.3mm, and 2h is kept the temperature at 1245 DEG C.It is surveyed after cooling Obtain the flexural strength and the coefficient of expansion of porcelain strip(Table 2).From the point of view of the amount of coloring oxide, MnO2And Cr2O3Amount it is identical, 7# Additional a little Fe in middle palm fibre glaze2O3, the more stable red α-Fe of colour generation can be precipitated in glaze2O3
The chemical composition of 2 three kinds of electroceramics palm fibre glaze of table(wt%)And physical property
The Thoughts of the present invention:Be transformed produce in it has proved that effective, ripe electroceramics glaze formula by way of, system Make inorganic adhesive glaze.Its method be exactly analysis have glaze ingredient and its role, then handle respectively again, then prepare it is suitable In the glaze of inorganic adhesive.
Electroceramics palm fibre glaze can be divided into three parts:As the parent glaze of glaze main part, with iron oxide, chromium oxide and manganese oxide etc. Based on colour generation oxide and other functional component.The feature for analyzing above-mentioned several glaze, has been divided into above-mentioned Three parts.Colour generation oxide is removed from glaze formula first, by the other raw materials of the primary raw material comprising colour generation oxide It substitutes(The raw material east fort mud of the Hunan Liling output of Tian Tuyong equivalent is substituted in this example, eastern fort mud and field soil at being respectively in In table 3), remaining is the parent glaze for eliminating pigmentation element.
The chemical composition (wt%) of 3 east Tian Tuyu fort mud of table
In parent glaze, then additional 3 parts of albites, 3 parts of boraxs, other raw materials remain unchanged, after being mixed uniformly, at 1450 DEG C The above melting, water quenching, are made parent glaze frit(Hereinafter referred to as frit), spare.
According to the ratio of the pigmentation element removed from former glaze formula, raw material is done with colour generation oxide, uses solid reaction process Synthesize colorant.In this example, it is feed proportioning that we, which use analytically pure iron oxide, manganese oxide and chromium oxide, is added a small amount of Magnesia and 3% borax, pass through solid state reaction kinetics toner at 1200 DEG C.The toner of synthesis is crushed again after cooling, mistake Sieve, pickling, drying, the spinel-type bronzing agent just synthesized.Brown material colour generation has certain variation range, with reference to above-mentioned The ratio of colour generation oxide, devises the formula of 2 toners in 3 glaze(It is shown in Table 4), synthesized 2 kinds of colorants.Synthesized color Material, can be used alone, can also be used in mixed way.
4 color base material of table matches(%)
Color base material formula Manganese oxide Iron oxide Chromium oxide
No01 75 12.5 12.5
No02 68.6 11.8 19.6
Using prepared parent glaze frit, the colorant of synthesis and the main zinc oxide for playing Nucleating Agent and zirconium oxide as function Property component is prepared for having certain crystallizing power and can form the inorganic adhesive glaze of continuous middle layer in surface between porcelain.
The ratio of the bronzing agent 8% that this example uses parent glaze frit 90%, synthesizes, zinc oxide and zircon each 1% weighs It is placed on afterwards using zirconium oxide or aluminium oxide as the ball of abrasive body(Sand)It is ground 12 hours or so in grinding machine, crosses 320 mesh sieve, control tails over No more than 0.5% to get it is a kind of new but with inorganic adhesive glaze similar in original glaze for electric porcelain ingredient.
Inorganic adhesive glaze is prepared using fritted glaze and synthesis toner, there are three main causes, exists first, can avoid glaze layer Occur the bubble for being difficult to exclude in melting process, second is that using the colorant of synthesis, also can avoid generating when colour generation oxide high-temperature Bubble;Third, Nucleating Agent is added, it can make that some crystalline phases are precipitated in glaze layer, adhesive strength can also be improved.In addition, in production Mature glaze for electric porcelain is transformed into inorganic adhesive glaze, it is ensured that the stability of the property of glaze increases inorganic adhesive success rate.With Under be using the electron scanning micrograph of inorganic adhesive powdered frit bonding hollow porcelain insulator, photo show, and glaze and porcelain body are Perfect adaptation has started that crystalline phase is precipitated in glaze.The bend loading of obtained product(It destroys)602kNm is reached, has shown to glue Connect excellent effect.
Embodiment 2
In order to discuss the effect of the powdered frit or glaze cream that apply inorganic adhesive glaze, the inorganic adhesive glaze of both forms is existed respectively Adhesive test has been carried out in the porcelain strip of identical plane interface.The notch and dress of strip, which are burnt, sees photo.
The dry method of directly upper powdered frit is respectively adopted and directly carries out glazing with the wet method of glaze cream.It is added to when with enamel frit makeing cream few The Ludox of amount, to enhance its cementability.Its flexural strength is measured after burning, to evaluate its adhesive effect(Table 5).
The flexural strength of 5 dry method of table flat nick porcelain strip Nian Jie with wet method(MPa)
Glazing mode 1 2 3 4 5 6 7 Average value
Dry method 70 75 73 69 75 65 68 71
Wet method intensity 86 84 80 79 77 84 90 83
From the point of view of the interface situation of glaze, the section part of dry method bonding, bubble is more and larger, and the section part of wet method bonding, Bubble is although more but universal all smaller, that is to say, that the adhesive glaze that wet method is bonded coupon interface is bonded more than dry method Uniformly, the effect for being also easier to control thus be bonded with glaze cream in technique is better than the effect being directly bonded with powdered frit.
The content that above-described embodiment illustrates should be understood as that these embodiments are only used for being illustrated more clearly that the present invention, without For limiting the scope of the invention, after having read the present invention, various equivalent forms of the those skilled in the art to the present invention Modification each fall within the application range as defined in the appended claims.

Claims (7)

1. a kind of preparation method of inorganic adhesive glaze, which is characterized in that include the following steps:
S1, parent glaze, borax and albite are mixed, is fired into parent glaze melt within the scope of 1200 DEG C~1500 DEG C, water quenching, Parent glaze frit is obtained, it is spare;
Wherein, the additive amount of borax is 2wt%~6wt% of basic glaze, and the additive amount of albite is 2wt%~8wt% of basic glaze;
S2, step S1 is obtained to parent glaze frit and Nucleating Agent mixing, grinding obtains inorganic adhesive glaze;
Wherein, the additive amount of the Nucleating Agent is 1wt%~5wt% of basic glaze frit.
2. the preparation method of inorganic adhesive glaze according to claim 1, which is characterized in that in step S2, step S1 is obtained Parent glaze frit, Nucleating Agent and coloring material for mixing are obtained, grinding obtains inorganic adhesive glaze.
3. the preparation method of inorganic adhesive glaze according to claim 2, which is characterized in that the preparation method of the colorant For:First basic toner, magnesia and borax are mixed, then keep the temperature 1 ~ 3h under the conditions of 900 ~ 1350 DEG C, is then cooled down, is ground, Successively after pickling, cleaning, drying obtains colorant;
Wherein, the additive amount of magnesia is 1 ~ 8wt% of basic toner, and the additive amount of borax is 1 ~ 10wt% of basic toner.
4. the preparation method of inorganic adhesive glaze according to claim 3, which is characterized in that the basis toner includes three oxygen Change two iron, chrome green, manganese dioxide.
5. the preparation method of inorganic adhesive glaze according to claim 1, which is characterized in that in parts by mass, the basis Glaze includes 10-18 parts of feldspar powder, 20-30 parts of silica flour, field master worker soil or mud 2-6 parts of Hubei, 8-15 parts of porcelain powder, calcite 2-8 Part, 1-3 parts of talcum powder, 0-3 parts of barium carbonate, 0-2 parts of spodumene.
6. the preparation method of inorganic adhesive glaze according to claim 1, which is characterized in that the Nucleating Agent includes oxidation Zinc, zirconium silicate, fluorite, kaolinic at least one.
7. a kind of inorganic adhesive glaze, which is characterized in that be made of preparation method as claimed in any one of claims 1 to 6.
CN201810427597.6A 2018-05-07 2018-05-07 Inorganic bonding glaze and preparation method thereof Active CN108516684B (en)

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CN112608028A (en) * 2020-12-31 2021-04-06 江苏南瓷绝缘子股份有限公司 High-strength suspension insulator head glaze and preparation method thereof

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CN110002868A (en) * 2019-04-28 2019-07-12 福建省德化县盛鼎瓷艺有限公司 A kind of anti-preparation method for breaking up ceramics
CN112608028A (en) * 2020-12-31 2021-04-06 江苏南瓷绝缘子股份有限公司 High-strength suspension insulator head glaze and preparation method thereof

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