CN103387382A - Ceramic corundum abrasive containing multiphase additive system and preparation method thereof - Google Patents
Ceramic corundum abrasive containing multiphase additive system and preparation method thereof Download PDFInfo
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- CN103387382A CN103387382A CN2013101050130A CN201310105013A CN103387382A CN 103387382 A CN103387382 A CN 103387382A CN 2013101050130 A CN2013101050130 A CN 2013101050130A CN 201310105013 A CN201310105013 A CN 201310105013A CN 103387382 A CN103387382 A CN 103387382A
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Abstract
The invention discloses a ceramic corundum abrasive containing a multiphase additive system and a preparation method thereof. According to the invention, a multiphase additive is introduced with 99.00 to 95.00% by mass of industrial aluminum nitrate used as a raw material; the multiphase additive system is introduced in the form of H3BO3, TEOS, Ba(NO3)2 and Cu(NO3)2. A sol-gel process is employed to prepare the ceramic corundum abrasive; ammonia water is used as a precipitating agent for preparation of a precursor, and then drying, sieving and calcining at a high temperature of 1200 to 1300 DEG C are carried out so as to obtain the ceramic corundum abrasive. Raw materials for the ceramic corundum abrasive are widely available and cheap; the used additive can substantially reduce sintering temperature, thereby reducing energy consumption; the obtained abrasive has a compact and uniform microscopic structure, single-particle compressive strength and grinding performance of the abrasive are improved, and the service life of the abrasive is prolonged.
Description
Technical field
The present invention relates to a kind of ground finish abrasive material and preparation method thereof, especially relate to a kind of New kind of ceramic Alumdu Grits (SG abrasive material) that contains the complex phase additive and preparation method thereof.
Background technology
Ceramic corundum abrasive material (being the SG abrasive material) is the high purity corundum abrasive that the micro crystal structure forms that has that adopts the sol-gel method preparation.Compare with common fused corundom abrasive material, not only hardness is high, and because abrasive particle is microlitic structure, have a lot of cleavage surfaces under external force only crystallite come off, and constantly produce new cutting edge, self-sharpening is good, and peels off less; With the grinding tool of ceramic corundum abrasive material preparation have that wear resistance is good, grinding heat is few, long service life, grinding ratio is large, resection rate is high and the advantage such as good grinding quality.The grinding tool for preparing well below superhard materials such as cubic boron nitride (CBN) and diamonds again on price simultaneously, and also not to the particular requirement of equipment for grinding, thereby, at key areas such as aerospace, be used widely now.
Although the ceramic corundum abrasive material has plurality of advantages, application prospect is extensive,, because the fusing point (2050 ℃) of pure alumina is very high, makes low temperature in preparation process be difficult to sintering, and excess Temperature easily causes again abnormal grain growth, destructive characteristics.Therefore how to reduce ceramic corundum abrasive material firing temperature, keeping again the homogeneity of its microstructure and pattern simultaneously is the emphasis of ceramic corundum abrasive material research field.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, based on colloidal sol-gel technique, adopt a kind of effective new additive agent system to reduce the firing temperature of ceramic corundum abrasive material, can realize that the abrasive material microscopic appearance is controlled, improve simultaneously product mechanics and grinding performance.
Technical purpose of the present invention is achieved by following technical proposals:
A kind of ceramic corundum abrasive material that contains the complex phase additive system and preparation method thereof, with industrial nitric acid aluminium Al (NO
3)
39H
2O is raw material, and the mass percent that the complex phase additive of introducing accounts for final abrasive material is 1.00～5.00%, described industrial nitric acid aluminium Al (NO
3)
39H
2The mass percent that O accounts for final abrasive material is 95-99%.
Described complex phase additive system is by tetraethoxy (TEOS), H
3BO
3, Ba (NO
3)
2And Cu (NO
3)
2Form, the mass fraction of each additive is: TEOS is 40～100 parts, and preferable range is 70～90 parts, is more preferably 70-85 parts; H
3BO
3Be 1～20 part, preferable range is 5～15 parts, is more preferably 5-10 parts; Ba (NO
3)
2Be 1～30 part, preferable range is 5～20 parts, is more preferably 10-15 parts; Cu (NO
3)
2Be 1～50 part, preferable range is 1～30 part, is more preferably 5-20 parts.
When being prepared, according to following step, carry out:
(1) utilize industrial nitric acid aluminium Al (NO
3)
39H
2O is the aluminum ions aqueous solution of raw material configuration, specifically, adopts industrial nitric acid aluminium Al (NO
3)
39H
2O is raw material, removes by filter impurity after water-soluble, is made into the aqueous solution that aluminium ion concentration is 0.2～0.4mol/L;
(2), with the aluminum ion aqueous gel of step (1) configuration, obtain Al (OH)
3Gel, specifically, splash into ammoniacal liquor in the aqueous solution of step (1), and stir and to make its complete gelation, regulates pH between 9～10, then suction filtration, wash to obtain Al (OH)
3Gel; Described ammoniacal liquor can be selected the concentration of 0.1-1mol/L, namely provides gel to generate needed alkaline environment;
(3) with the Al (OH) of step (2) preparation
3After mixing, gel and complex phase additive prepare xerogel, specifically, the complex phase additive is added in the gel of step (2) according to above-mentioned mass percent, it is fully mixed with the corundum abrading-ball take ethanol as medium, then mixture is obtained xerogel after drying under 60 ℃ is sloughed moisture content and/or other solvents, then sieve the acquisition dry gel particle;
(4) xerogel of step (3) preparation is calcined, prepare corundum abrasive, specifically, dry gel particle in step (3) is calcined under the condition of 1200～1300 ℃, soaking time is 0.5-2h, wait burn till be cooled to room temperature (20-25 ℃) after again through the screening can obtain varigrained corundum abrasive
The abrasive material of preparation is carried out Electronic Speculum pattern and XRD characterizes, with reference to the accompanying drawings shown in, can obtain in the sample abrasive material with the standard card contrast is all α-Al
2O
3Crystalline phase (corundum); The corundum abrasive internal microstructure is the tabular or compact reactor cumuliformis of Polygons, and final abrasive material shape is controlled; Abrasive material internal microstructure grain-size is between 200～500nm.The gained abrasive material is carried out the single particle intensity test, use ZCM-II type diamond isostatic pressing strength tester, represent with newton (N), choosing 40 particles between 60～80 orders tests, use its mean value as its single particle strength value, and test result is more than the mean value of single particle ultimate compression strength can reach 55N.
Compared with prior art, enlarged the additive range of choice of corundum abrasive in technical scheme of the present invention, the additive wide material sources, can effectively reduce the sintering temperature of corundum abrasive, improve single particle ultimate compression strength, the impelling strength of corundum abrasive, thereby reduced production cost, reduced energy consumption, simultaneously further optimized internal microstructure, made its grain-size between 200～500nm.
Description of drawings
The pattern photo (field emission scanning electron microscope, FESEM, JEOLJSM-6700F) of Fig. 1 corundum abrasive of the present invention.
The XRD spectral line of Fig. 2 corundum abrasive of the present invention (RIGAKU/DMAX2500, Rigaku meeting).
Embodiment
The invention will be further described below in conjunction with specific embodiment.
It is raw material that following embodiment of the present invention all adopts industrial nitric acid aluminium, and the ammoniacal liquor of 0.1mol/L is precipitation agent, and following table is seen in the source of each raw material for details.
Table 1 raw material manufacturer form
At first can take raw material according to the stoichiometric ratio of the complex phase additive shown in following table, mix rear standbyly, every part is 0.1g
The stoichiometric ratio of table 2 complex phase additive
| NO. | TEOS/ part | H 3BO 3/ part | Ba(NO 3) 2/ part | Cu(NO
3)
2/ |
| 1 | 90 | 3 | 7 | 7 |
| 2 | 90 | 5 | 8 | 15 |
| 3 | 78 | 7 | 10 | 25 |
| 4 | 60 | 10 | 14 | 20 |
| 5 | 48 | 8 | 24 | 36 |
| 6 | 37 | 9 | 28 | 40 |
| 7 | 40 | 1 | 15 | 1 |
| 8 | 100 | 20 | 30 | 50 |
| 9 | 70 | 15 | 1 | 5 |
| 10 | 85 | 10 | 20 | 30 |
Below as an example of preparation 4g corundum abrasive example, describe, take the 4g corundum abrasive as the benchmark raw materials weighing, the complex phase additives ratio is that the mass percent of final abrasive material is 1～5.00%, and all the other are industrial nitric acid aluminium Al (NO
3)
39H
2O。
At first industrial nitric acid aluminium is water-soluble, elimination impurity also is made into the solution that aluminium ion concentration is 0.2mol/L;
Splash into ammoniacal liquor in above-mentioned solution, and stir and to make its complete gelation, regulating the pH value is 9.3, then through suction filtration, wash to obtain Al (OH)
3Wet gel;
No. 1 complex phase additive in table 2 (add-on be final abrasive material quality 1%) is added Al (OH)
3In wet gel, take ethanol as medium, with the corundum abrading-ball, it is fully mixed;
The wet gel that will contain additive is dry under 60 ℃, obtains after xerogel sieving obtaining dry gel particle again;
With the Al (OH) that sieves and classification obtains
3Dry gel particle is calcined under 1300 ℃, insulation 1.5h, naturally cool to room temperature, more further screening obtains varigrained New kind of ceramic Alumdu Grits.
Embodiment 2
At first industrial nitric acid aluminium is water-soluble, elimination impurity also is made into the aqueous solution that aluminium ion concentration is 0.4mol/L;
Splash into ammoniacal liquor in above-mentioned solution, and stir and to make its complete gelation, regulating the pH value is 9.5, then through suction filtration, wash to obtain Al (OH)
3Wet gel;
No. 3 complex phase additives in table 2 (add-on be final abrasive material quality 2.5%) are added Al (OH)
3In wet gel, take ethanol as medium, with the corundum abrading-ball, it is fully mixed;
The wet gel that will contain additive is dry under 60 ℃, obtains after xerogel sieving obtaining dry gel particle again;
With the Al (OH) that sieves and classification obtains
3Dry gel particle is calcined under 1200 ℃, insulation 1h, naturally cool to room temperature, more further screening obtains varigrained New kind of ceramic Alumdu Grits.
Embodiment 3
At first industrial nitric acid aluminium is water-soluble, elimination impurity also is made into the aqueous solution that aluminium ion concentration is 0.25mol/L;
Splash into ammoniacal liquor in above-mentioned solution, and stir and to make its complete gelation, regulating the pH value is 9.5, then through suction filtration, wash to obtain Al (OH)
3Wet gel;
No. 5 complex phase additives in table 2 (add-on be final abrasive material quality 5%) are added Al (OH)
3In wet gel, take ethanol as medium, with the corundum abrading-ball, it is fully mixed;
The wet gel that will contain additive is dry under 60 ℃, obtains after xerogel sieving obtaining dry gel particle again;
With the Al (OH) that sieves and classification obtains
3Dry gel particle is calcined under 1250 ℃, insulation 2h, naturally cool to room temperature, more further screening obtains varigrained New kind of ceramic Alumdu Grits.
Embodiment 4
At first industrial nitric acid aluminium is water-soluble, elimination impurity also is made into the aqueous solution that aluminium ion concentration is 0.35mol/L;
Splash into ammoniacal liquor in above-mentioned solution, and stir and to make its complete gelation, regulating the pH value is 9.0, then through suction filtration, wash to obtain Al (OH)
3Wet gel;
No. 7 complex phase additives in table 2 (add-on be final abrasive material quality 3%) are added Al (OH)
3In wet gel, take ethanol as medium, with the corundum abrading-ball, it is fully mixed;
The wet gel that will contain additive is dry under 60 ℃, obtains after xerogel sieving obtaining dry gel particle again;
With the Al (OH) that sieves and classification obtains
3Dry gel particle is calcined under 1250 ℃, insulation 0.5h, naturally cool to room temperature, more further screening obtains varigrained New kind of ceramic Alumdu Grits.
Embodiment 5
At first industrial nitric acid aluminium is water-soluble, elimination impurity also is made into the aqueous solution that aluminium ion concentration is 0.3mol/L;
Splash into ammoniacal liquor in above-mentioned solution, and stir and to make its complete gelation, regulating the pH value is 10, then through suction filtration, wash to obtain Al (OH) 3 wet gels;
No. 10 complex phase additives in table 2 (add-on be final abrasive material quality 2%) are added Al (OH)
3In wet gel, take ethanol as medium, with the corundum abrading-ball, it is fully mixed;
The wet gel that will contain additive is dry under 60 ℃, obtains after xerogel sieving obtaining dry gel particle again;
With the Al (OH) that sieves and classification obtains
3Dry gel particle is calcined under 1250 ℃, insulation 2h, naturally cool to room temperature, more further screening obtains varigrained New kind of ceramic Alumdu Grits.
Above the present invention has been done exemplary description; should be noted that; in the situation that do not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (10)
1. a ceramic corundum abrasive material that contains the complex phase additive system, is characterized in that, crystalline phase is α-Al
2O
3, grain-size is between 200～500nm, with industrial nitric acid aluminium Al (NO
3)
39H
2O is raw material, and the mass percent that the complex phase additive of introducing accounts for final abrasive material is 1.00～5.00%, described industrial nitric acid aluminium Al (NO
3)
39H
2The mass percent that O accounts for final abrasive material is 95-99%; Described complex phase additive system is by tetraethoxy, H
3BO
3, Ba (NO
3)
2And Cu (NO
3)
2Form, the mass fraction of each additive is: tetraethoxy is 40～100 parts, H
3BO
3Be 1～20 part, Ba (NO
3)
2Be 1～30 part, Cu (NO
3)
2It is 1～50 part; Carry out according to following step:
(1) utilize industrial nitric acid aluminium Al (NO
3)
39H
2O is the aluminum ions aqueous solution of raw material configuration;
(2), with the aluminum ion aqueous gel of step (1) configuration, obtain Al (OH)
3Gel;
(3) with the Al (OH) of step (2) preparation
3After mixing, gel and complex phase additive prepare xerogel;
(4) dry gel particle in step (3) is calcined under the condition of 1200～1300 ℃, soaking time is 0.5-2h, wait burn till be cooled to room temperature (20-25 ℃) after again through the screening can obtain varigrained corundum abrasive.
2. a kind of ceramic corundum abrasive material that contains the complex phase additive system according to claim 1, is characterized in that, in described complex phase additive system, the tetraethoxy preferable range is 70～90 parts, H
3BO
3Preferable range is 5～15 parts, Ba (NO
3)
2Preferable range is 5～20 parts, Cu (NO
3)
2Preferable range is 1～30 part.
3. a kind of ceramic corundum abrasive material that contains the complex phase additive system according to claim 1, is characterized in that, in described complex phase additive system, and preferred 70-85 parts of tetraethoxy, H
3BO
3Preferred 5-10 parts, Ba (NO
3)
2Preferred 10-15 parts, Cu (NO
3)
2Preferred 5-20 parts.
4. a kind of ceramic corundum abrasive material that contains the complex phase additive system according to claim 1, is characterized in that, described preparation process is as follows specifically:
(1) adopt industrial nitric acid aluminium Al (NO
3)
39H
2O is raw material, removes by filter impurity after water-soluble, is made into the aqueous solution that aluminium ion concentration is 0.2～0.4mol/L;
(2) splash into ammoniacal liquor in the aqueous solution of step (1), and stir and to make its complete gelation, regulate pH between 9～10, then suction filtration, wash to obtain Al (OH)
3Gel;
(3) the complex phase additive is added in the gel of step (2), take ethanol as medium, with the corundum abrading-ball, it is fully mixed, then mixture is obtained xerogel after drying under 60 ℃ is sloughed moisture content and/or other solvents, then sieve the acquisition dry gel particle;
(4) dry gel particle in step (3) is calcined under the condition of 1200～1300 ℃, soaking time is 0.5-2h, wait burn till be cooled to room temperature (20-25 ℃) after again through the screening can obtain varigrained corundum abrasive.
5. a kind of ceramic corundum abrasive material that contains the complex phase additive system according to claim 1, is characterized in that, in described step (2), described ammoniacal liquor can be selected the concentration of 0.1-1mol/L, namely provides gel to generate needed alkaline environment.
6. a preparation method who contains the ceramic corundum abrasive material of complex phase additive system, is characterized in that, with industrial nitric acid aluminium Al (NO
3)
39H
2O is raw material, and the mass percent that the complex phase additive of introducing accounts for final abrasive material is 1.00～5.00%, described industrial nitric acid aluminium Al (NO
3)
39H
2The mass percent that O accounts for final abrasive material is 95-99%; Described complex phase additive system is by tetraethoxy, H
3BO
3, Ba (NO
3)
2And Cu (NO
3)
2Form, the mass fraction of each additive is: tetraethoxy is 40～100 parts, H
3BO
3Be 1～20 part, Ba (NO
3)
2Be 1～30 part, Cu (NO
3)
2It is 1～50 part; Carry out according to following step:
(1) utilize industrial nitric acid aluminium Al (NO
3)
39H
2O is the aluminum ions aqueous solution of raw material configuration;
(2), with the aluminum ion aqueous gel of step (1) configuration, obtain Al (OH)
3Gel;
(3) with the Al (OH) of step (2) preparation
3After mixing, gel and complex phase additive prepare xerogel;
(4) dry gel particle in step (3) is calcined under the condition of 1200～1300 ℃, soaking time is 0.5-2h, wait burn till be cooled to room temperature (20-25 ℃) after again through the screening can obtain varigrained corundum abrasive.
7. a kind of preparation method who contains the ceramic corundum abrasive material of complex phase additive system according to claim 6, is characterized in that, in described complex phase additive system, the tetraethoxy preferable range is 70～90 parts, H
3BO
3Preferable range is 5～15 parts, Ba (NO
3)
2Preferable range is 5～20 parts, Cu (NO
3)
2Preferable range is 1～30 part.
8. a kind of preparation method who contains the ceramic corundum abrasive material of complex phase additive system according to claim 6, is characterized in that, in described complex phase additive system, and preferred 70-85 parts of tetraethoxy, H
3BO
3Preferred 5-10 parts, Ba (NO
3)
2Preferred 10-15 parts, Cu (NO
3)
2Preferred 5-20 parts.
9. a kind of preparation method who contains the ceramic corundum abrasive material of complex phase additive system according to claim 6, is characterized in that, described preparation process is as follows specifically:
(1) adopt industrial nitric acid aluminium Al (NO
3)
39H
2O is raw material, removes by filter impurity after water-soluble, is made into the aqueous solution that aluminium ion concentration is 0.2～0.4mol/L;
(2) splash into ammoniacal liquor in the aqueous solution of step (1), and stir and to make its complete gelation, regulate pH between 9～10, then suction filtration, wash to obtain Al (OH)
3Gel;
(3) the complex phase additive is added in the gel of step (2), take ethanol as medium, with the corundum abrading-ball, it is fully mixed, then mixture is obtained xerogel after drying under 60 ℃ is sloughed moisture content and/or other solvents, then sieve the acquisition dry gel particle;
(4) dry gel particle in step (3) is calcined under the condition of 1200～1300 ℃, soaking time is 0.5-2h, wait burn till be cooled to room temperature (20-25 ℃) after again through the screening can obtain varigrained corundum abrasive.
10. a kind of preparation method who contains the ceramic corundum abrasive material of complex phase additive system according to claim 6, it is characterized in that, in described step (2), described ammoniacal liquor can be selected the concentration of 0.1-1mol/L, namely provides gel to generate needed alkaline environment.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966705A (en) * | 2017-03-15 | 2017-07-21 | 天津大学 | A kind of nanocrystalline ceramics corundum abrasive containing complex phase additive |
| CN107814560A (en) * | 2017-09-30 | 2018-03-20 | 江苏金石研磨有限公司 | A kind of ceramic grinding ball rolls shaping composite fortifier and preparation method thereof and its application method |
| CN110054482A (en) * | 2019-03-18 | 2019-07-26 | 山东天汇研磨耐磨技术开发有限公司 | A kind of machine tool industry synchronous modification of microcrystalline ceramic abrasive and its manufacturing method |
| CN113845356A (en) * | 2021-10-22 | 2021-12-28 | 湖南约瑟夫科技有限公司 | Ceramic corundum abrasive material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732214A (en) * | 2012-06-20 | 2012-10-17 | 天津大学 | Ceramic corundum abrasive containing multiphase additive |
| CN102775135A (en) * | 2012-07-11 | 2012-11-14 | 天津大学 | Novel ceramic corundum abrasive |
-
2013
- 2013-03-28 CN CN2013101050130A patent/CN103387382A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732214A (en) * | 2012-06-20 | 2012-10-17 | 天津大学 | Ceramic corundum abrasive containing multiphase additive |
| CN102775135A (en) * | 2012-07-11 | 2012-11-14 | 天津大学 | Novel ceramic corundum abrasive |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106966705A (en) * | 2017-03-15 | 2017-07-21 | 天津大学 | A kind of nanocrystalline ceramics corundum abrasive containing complex phase additive |
| CN107814560A (en) * | 2017-09-30 | 2018-03-20 | 江苏金石研磨有限公司 | A kind of ceramic grinding ball rolls shaping composite fortifier and preparation method thereof and its application method |
| CN110054482A (en) * | 2019-03-18 | 2019-07-26 | 山东天汇研磨耐磨技术开发有限公司 | A kind of machine tool industry synchronous modification of microcrystalline ceramic abrasive and its manufacturing method |
| CN113845356A (en) * | 2021-10-22 | 2021-12-28 | 湖南约瑟夫科技有限公司 | Ceramic corundum abrasive material and preparation method and application thereof |
| CN113845356B (en) * | 2021-10-22 | 2022-11-29 | 湖南约瑟夫科技有限公司 | Ceramic corundum abrasive material and preparation method and application thereof |
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Application publication date: 20131113 |