CN110204358A - A kind of ceramics pretreatment fluid and preprocess method - Google Patents
A kind of ceramics pretreatment fluid and preprocess method Download PDFInfo
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- CN110204358A CN110204358A CN201910561931.1A CN201910561931A CN110204358A CN 110204358 A CN110204358 A CN 110204358A CN 201910561931 A CN201910561931 A CN 201910561931A CN 110204358 A CN110204358 A CN 110204358A
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Abstract
The invention discloses a kind of ceramic pretreatment fluids, and preparing raw material includes etchant, pH buffer, pH adjusting agent, and solvent is water.The invention also discloses a kind of ceramic preprocess methods comprising the steps of: oil removing, table tune, preimpregnation, pretreatment.There is equally distributed micropore using the present invention treated ceramic surface, be used to prepare the ceramic composite compound with plastics, rubber, coating, it is compound after binding force between different materials it is strong, the whole air-tightness of composite material is good.
Description
Technical field
The present invention relates to ceramic material field more particularly to a kind of ceramic pretreatment fluids and preprocess method.
Background technique
Ceramic material is that have high-melting-point, high rigidity, high abrasion using extremely wide a kind of inorganic non-metallic material
The advantages that property, resistance to oxidation, but its disadvantage is also fairly obvious, such as tensile strength is low, plasticity and toughness are very poor.Composite material
Compound each material is participated in by two or more compound different materials to realize the effect maximized favourable factors and minimized unfavourable ones
Advantage can embody in the composite, and disadvantage can also make up mutually, therefore can be with by the way that composite material is made in ceramics
The deficiencies of improving ceramic plasticity, poor toughness.
Since ceramics are inorganic non-metallic material, main component is silica, silicate etc., when compound with other materials
When, it is such as compound with plastics, rubber, coating etc. especially with high molecular material, it is poor often to will appear binding force between material
The problem of, in the field for having demand to composite material air-tightness, ceramic composite is also difficult to reach using standard.
Summary of the invention
To solve the above-mentioned problems, the first aspect of the present invention provides a kind of ceramic pretreatment fluid, prepares raw material packet
Containing etchant, pH buffer, pH adjusting agent, solvent is water.
As a kind of perferred technical scheme, the concentration of the etchant is 75~125g/L, and the concentration of pH buffer is
15~45g/L.
As a kind of perferred technical scheme, the pH of the ceramic pretreatment fluid is 3~5.
As a kind of perferred technical scheme, the etchant is fluoride.
As a kind of perferred technical scheme, the fluoride is in hydrofluoric acid, potassium fluoride, ammonium acid fluoride, sodium fluoride
One or more mixing.
As a kind of perferred technical scheme, the pH buffer is phosphate.
As a kind of perferred technical scheme, the phosphate is selected from sodium phosphate, potassium phosphate, disodium-hydrogen, phosphoric acid one
One of hydrogen potassium, sodium dihydrogen phosphate, potassium dihydrogen phosphate or a variety of mixing.
The second aspect of the present invention provides a kind of ceramic preprocess method using above-mentioned ceramic pretreatment fluid, comprising with
Lower step:
A. it oil removing: is washed after ceramics are carried out ultrasonic wave acid deoiling；
B. table tune: it will wash after ceramic ultrasonic wave cleaning that step a is obtained, then handled using table adjustment；
C. presoak: the ceramics that step b is obtained presoak in sulfuric acid solution, then wash；
D. it pre-processes: step c being obtained into ceramics and is handled using above-mentioned ceramic pretreatment fluid, then is washed, is then neutralized,
It is dried after washing twice, ceramics pretreatment is completed.
The third aspect of the present invention provides a kind of pretreated ceramics, is using above-mentioned ceramic preprocess method
What processing obtained.
The fourth aspect of the present invention provides a kind of ceramic composite, is with above-mentioned pretreated ceramics for base
Body, with plastics, rubber, the compound ceramic composite obtained of coating.
The utility model has the advantages that a kind of ceramic pretreatment fluid provided by the invention and pretreatment mode are used for the pottery of ceramic composite
The pretreatment of porcelain basal body, treated ceramic surface there are a large amount of equally distributed micropores and one layer of nitrogenous organic transformation film,
Should treated ceramics with other materials compound tense can be provided simultaneously with physics riveted power and Chemical bonding, improve material it
Between binding force and composite material entirety air-tightness；In addition, ceramics pretreatment fluid provided by the invention can also be to surface micropore
Size is adjusted, and then adjusts the binding force of composite material, to meet different field to the various demands of composite material.
Detailed description of the invention
In order to further explain the beneficial effect of a kind of ceramic pretreatment fluid and preprocess method provided in the present invention
Fruit provides corresponding attached drawing, it is pointed out that attached drawing provided in the present invention be elected in all attached drawings it is individual
Example, purpose are also not as limitations on the claims, all corresponding by other of attached drawing acquisition provided herein
Map is it is believed that within the scope of the application protection.
Fig. 1 is that the embodiment of the present application 3 is used for the pretreated effect of ceramics, and legend is 10.0 μm.
Fig. 2 is that the embodiment of the present application 1 is used for the pretreated effect of ceramics, and legend is 10.0 μm.
Specific embodiment
In conjunction with preferred implementation method of the invention below detailed description and including embodiment can be further understood that this hair
Bright content.Unless otherwise indicated, all technologies used herein and scientific term all have general with the application fields
Logical technical staff's is generally understood identical meaning.If mentioned in the definition and the application of the concrete term disclosed in the prior art
Any definition supplied is inconsistent, then term provided herein of being subject to defines.
It is used in the present context, unless being clearly dictated in context, otherwise without the spy of the single plural form of restriction
Sign is also intended to the feature including plural form.It will also be appreciated that term as used herein " by ... preparation " it is synonymous with "comprising",
" comprising ", " including ", " having ", "comprising" and/or " including " indicate stated group when used in this manual
Object, step, method, product or device are closed, but does not preclude the presence or addition of one or more of the other composition, step, method, system
Product or device.In addition, using " preferred ", " preferably ", " preferred " etc. to be when describing presently filed embodiment
Refer to, can provide the embodiment of the present invention of certain beneficial effects in some cases.However, under identical circumstances or other feelings
Under condition, other embodiments are also likely to be preferred.In addition to this, not dark to the statement of one or more preferred embodiments
Show that other embodiments are unavailable, is also not intended to exclude other embodiments except the scope of the present invention.
To solve the above-mentioned problems, the first aspect of the present invention provides a kind of ceramic pretreatment fluid, prepares raw material packet
Containing etchant, pH buffer, pH adjusting agent, solvent is water.
In some preferred embodiments, the concentration of the etchant is 75~125g/L, and the concentration of pH buffer is
15~45g/L.
In some preferred embodiments, the concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/
L。
Etchant
Etchant in the application manufactures micropore for corroding ceramic surface.Ceramics main component be silica and
Silicate, performance is highly stable, specific corrosive agent can only be used to be etched.
In some preferred embodiments, the etchant is fluoride.
In some preferred embodiments, the fluoride is in hydrofluoric acid, potassium fluoride, ammonium acid fluoride, sodium fluoride
One or more mixing；It is further preferred that the fluoride is ammonium acid fluoride.
PH buffer
PH buffer in the application can make hydrogen ion concentration in system keep stablizing, and then guarantee ceramic pretreatment fluid
Stability in use process.
In some preferred embodiments, the pH buffer is phosphate.
In some preferred embodiments, the phosphate is selected from sodium phosphate, potassium phosphate, disodium-hydrogen, phosphoric acid one
One of hydrogen potassium, sodium dihydrogen phosphate, potassium dihydrogen phosphate or a variety of mixing；It is further preferred that the phosphate is phosphoric acid
Sodium dihydrogen.
PH adjusting agent
PH adjusting agent in the application provides enough hydrogen ions for system, to participate in the corrosion reaction of ceramic surface.
In some preferred embodiments, the pH adjusting agent is organic acid.
In some preferred embodiments, the organic acid is selected from acetic acid, formic acid, citric acid, malic acid, Vitamin C
One of acid, tartaric acid, ethanedioic acid, malonic acid or a variety of mixing；It is further preferred that the organic acid is acetic acid.
In some preferred embodiments, the pH of the ceramic pretreatment fluid is 3~5；It is further preferred that the pottery
The pH of porcelain pretreatment fluid is 4.
In some preferred embodiments, the preparation method of the ceramic pretreatment fluid is comprised the steps of: to prepare
For 1L solution, weigh 75~125g of etchant, 15~45g of pH buffer is dissolved in 700mL water, stir evenly, be added pH tune
Agent is saved, pH value is adjusted to after 3~5, water is added to complement to 1L.
In some preferred embodiments, the preparation method of the ceramic pretreatment fluid is comprised the steps of: to prepare
For 1L solution, weigh etchant 100g, pH buffer 30g is dissolved in 700mL water, stir evenly, be added pH adjusting agent, adjust
PH value adds water to complement to 1L to after 4.
It has been found that selecting specific etchant that the pore-forming effect of stability and high efficiency may be implemented, this is because hydrogen fluoride
Ammonium is that substep ionizes in water, can slow down the process of corrosion reaction, make ceramic surface that will not be corroded excessively, leave mottled
Surface, ammonium ion therein can also adhere on the surface, form organic nitrogen-containing conversion film, molten with the progress of corrosion reaction
Hydrogen ion in liquid is constantly consumed, and will affect the acid-base property of system, after reaction carries out a period of time, treatment effect gradually becomes
Difference carries out reversible ionization reaction according to pH value of solution variation to the being adapted to property of addition of pH buffer, the hydrogen in maintenance system
Ion concentration, and pH adjusting agent a large amount of corrosion reactions can be provided needed for hydrogen ion, guarantee pore forming process can go on smoothly,
Improve pretreatment efficiency.Under etchant, pH buffer, the synergistic effect of pH adjusting agent, pretreated ceramic surface has
Be uniformly distributed, the aperture that size is controllable and one layer of nitrogenous organic transformation film, when as matrices of composite material, the surface and its
He has physics riveted power and Chemical bonding between material, therefore the ceramic composite has excellent binding force gentle
Close property.
The second aspect of the present invention provides a kind of ceramic preprocess method using above-mentioned ceramic pretreatment fluid, comprising with
Lower step:
A. it oil removing: is washed after ceramics are carried out ultrasonic wave acid deoiling；
B. table tune: it will wash after ceramic ultrasonic wave cleaning that step a is obtained, then handled using table adjustment；
C. presoak: the ceramics that step b is obtained presoak in sulfuric acid solution, then wash；
D. it pre-processes: step c being obtained into ceramics and is handled using above-mentioned ceramic pretreatment fluid, then is washed, is then neutralized,
It is dried after washing twice, ceramics pretreatment is completed.
The oil removing of preprocess method, table tune, preimpregnation, pretreatment operation may each be any art technology in the present invention
The common mode of operation of personnel.
In some preferred embodiments, in the step c sulfuric acid solution concentration be 80g/L, preimpregnation the time be
2min。
The third aspect of the present invention provides a kind of pretreated ceramics, is using above-mentioned ceramic preprocess method
What processing obtained.
The fourth aspect of the present invention provides a kind of ceramic composite, is with above-mentioned pretreated ceramics for base
Body, with plastics, rubber, the compound ceramic composite obtained of coating.
Embodiment
Technical solution of the present invention is described in detail by the following examples, but protection scope of the present invention is not limited to
In the embodiment.Raw material use herein is unless otherwise specified commercially available.
Embodiment 1
Embodiment 1 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride (No. CAS: 1341-49-7)；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate (No. CAS: 7558-80-7)；
The pH adjusting agent is acetic acid (No. CAS: 64-19-7)；
The pH of the ceramics pretreatment fluid is 4.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid comprising the steps of: for preparing 1L solution,
Weigh etchant 100g, pH buffer 30g is dissolved in 700mL water, is stirred evenly, and pH adjusting agent is added, adjust pH value to after 4,
Water is added to complement to 1L.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid comprising the steps of:
A. it oil removing: is washed after ceramics are carried out ultrasonic wave acid deoiling；
B. table tune: it will wash after ceramic ultrasonic wave cleaning that step a is obtained, then handled using table adjustment；
C. presoak: the ceramics that step b is obtained presoak 2min in the sulfuric acid solution of concentration 80g/L, then wash；
D. it pre-processes: step c being obtained into ceramics and is handled using above-mentioned ceramic pretreatment fluid, then is washed, is then neutralized,
It is dried after washing twice, ceramics pretreatment is completed.
Embodiment 2
Embodiment 2 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 3.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid comprising the steps of: for preparing 1L solution,
Weigh etchant 100g, pH buffer 30g is dissolved in 700mL water, is stirred evenly, and pH adjusting agent is added, adjust pH value to after 3,
Water is added to complement to 1L.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 3
Embodiment 3 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 5.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid comprising the steps of: for preparing 1L solution,
Weigh etchant 100g, pH buffer 30g is dissolved in 700mL water, is stirred evenly, and pH adjusting agent is added, adjust pH value to after 5,
Water is added to complement to 1L.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 4
Embodiment 4 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 75g/L, and the concentration of pH buffer is 15g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 4.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid comprising the steps of: for preparing 1L solution,
Weigh etchant 75g, pH buffer 15g is dissolved in 700mL water, is stirred evenly, and pH adjusting agent is added, adjust pH value to after 3, add
Water complements to 1L.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 5
Embodiment 5 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 125g/L, and the concentration of pH buffer is 45g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 4.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid comprising the steps of: for preparing 1L solution,
Weigh etchant 125g, pH buffer 45g is dissolved in 700mL water, is stirred evenly, and pH adjusting agent is added, adjust pH value to after 3,
Water is added to complement to 1L.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 6
Embodiment 6 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is potassium fluoride (No. CAS: 7789-23-3)；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 4.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid, similar to Example 1.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 7
Embodiment 7 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is disodium-hydrogen (No. CAS: 7558-79-4)；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 4.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid, similar to Example 1.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 8
Embodiment 8 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate；
The pH adjusting agent is citric acid (No. CAS: 77-92-9)；
The pH of the ceramics pretreatment fluid is 4.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid, similar to Example 1.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 9
Embodiment 9 provides a kind of ceramic pretreatment fluid, prepares raw material and includes etchant, pH buffer, pH adjusting agent,
Solvent is water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is sodium phosphate (No. CAS: 7601-54-9)；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 4.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid, similar to Example 1.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Embodiment 10
Embodiment 10 provides a kind of ceramic pretreatment fluid, and preparing raw material includes etchant, pH buffer, pH adjusting
Agent, solvent are water；
The concentration of the etchant is 100g/L, and the concentration of pH buffer is 30g/L；
The etchant is fluoride；The fluoride is ammonium acid fluoride；
The pH buffer is phosphate；The phosphate is sodium dihydrogen phosphate；
The pH adjusting agent is acetic acid；
The pH of the ceramics pretreatment fluid is 2.
This example additionally provides the preparation method of above-mentioned ceramic pretreatment fluid comprising the steps of: for preparing 1L solution,
Weigh etchant 100g, pH buffer 30g is dissolved in 700mL water, is stirred evenly, and pH adjusting agent is added, adjust pH value to after 2,
Water is added to complement to 1L.
This example additionally provides the ceramic preprocess method using above-mentioned ceramic pretreatment fluid, similar to Example 1.
Performance evaluation
Pretreated ceramics obtained to Examples 1 to 10 carry out performance evaluation, and Appreciation gist is ceramic surface
SEM photograph, evaluation content are the average pore size and average hole depth of ceramic surface micropore, the results are shown in Table 1.
Table 1
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Aperture/μm | 15 | 20 | 10 | 5 | 30 | 55 | 10 | 25 | 10 | 65 |
| Hole depth/μm | 10 | 15 | 5 | 5 | 25 | 40 | 5 | 15 | 5 | 60 |
By comparative example 1~10 it is known that ceramics pretreatment fluid provided by the invention and preprocess method can be with
A large amount of equally distributed micropores, and size adjustable are manufactured in ceramic surface, the composite material made using the ceramics as matrix can
With excellent binding force and air-tightness, the use scope of ceramic material is expanded.
At last it is pointed out that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not intended to limit the invention, it is all at this
Made any modifications, equivalent replacements, and improvements etc., should be included in protection model of the invention within the spirit and principle of invention
Within enclosing.
Claims (10)
1. a kind of ceramics pretreatment fluid, which is characterized in that it includes etchant, pH buffer, pH adjusting agent, solvent that it, which prepares raw material,
For water.
2. ceramics pretreatment fluid as described in claim 1, which is characterized in that the concentration of the etchant is 75~125g/L,
The concentration of pH buffer is 15~45g/L.
3. ceramics pretreatment fluid as claimed in claim 1 or 2, which is characterized in that the pH of the ceramics pretreatment fluid is 3~5.
4. ceramics pretreatment fluid as claimed in any one of claims 1 to 3, which is characterized in that the etchant is fluoride.
5. ceramics pretreatment fluid as claimed in claim 4, which is characterized in that the fluoride is selected from hydrofluoric acid, potassium fluoride, fluorine
Change one of hydrogen ammonium, sodium fluoride or a variety of mixing.
6. ceramics pretreatment fluid as claimed in any one of claims 1 to 3, which is characterized in that the pH buffer is phosphate.
7. ceramics pretreatment fluid as claimed in claim 6, which is characterized in that the phosphate is selected from sodium phosphate, potassium phosphate, phosphorus
One of a sour hydrogen sodium, potassium phosphate,monobasic, sodium dihydrogen phosphate, potassium dihydrogen phosphate or a variety of mixing.
8. a kind of ceramic preprocess method using pretreatment fluid ceramic as described in any one of claim 1~7, feature exist
In comprising the steps of:
A. it oil removing: is washed after ceramics are carried out ultrasonic wave acid deoiling；
B. table tune: it will wash after ceramic ultrasonic wave cleaning that step a is obtained, then handled using table adjustment；
C. presoak: the ceramics that step b is obtained presoak in sulfuric acid solution, then wash；
D. it pre-processes: step c being obtained into ceramics and is handled using pretreatment fluid ceramic as described in any one of claim 1~7,
It washes, then neutralizes again, dried after washing twice, ceramics pretreatment is completed.
9. a kind of pretreated ceramics, which is characterized in that it is using at ceramic preprocess method as claimed in claim 8
What reason obtained.
10. a kind of ceramic composite, which is characterized in that it is with pretreated ceramics as claimed in claim 9 for base
Body, with plastics, rubber, the compound ceramic composite obtained of coating.
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| CN114425835A (en) * | 2020-10-29 | 2022-05-03 | 比亚迪股份有限公司 | Ceramic matrix, ceramic plastic composite and preparation method thereof |
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| CN109023370A (en) * | 2018-08-30 | 2018-12-18 | 深圳市华星光电技术有限公司 | Etching solution and engraving method for copper-molybdenum metallic diaphragm |
| CN109112545A (en) * | 2018-09-25 | 2019-01-01 | 惠州市宙邦化工有限公司 | A kind of chemical etching composition of copper-molybdenum alloy film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114425835A (en) * | 2020-10-29 | 2022-05-03 | 比亚迪股份有限公司 | Ceramic matrix, ceramic plastic composite and preparation method thereof |
| CN114425835B (en) * | 2020-10-29 | 2023-08-08 | 比亚迪股份有限公司 | Ceramic matrix, ceramic plastic composite and preparation method thereof |
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