CN101740151B - Gel-casting method of Al2O3-B4C material - Google Patents

Abstract

The invention discloses a gel-casting method of an Al2O3-B4C material which belongs to nuclear fuel and is used for a pressurized water reactor in a nuclear power station. The method comprises the steps of: mixing N-hydroxymethyl acrylamide, methylenebisacrylamide and ammonium polyacrylate with deionized water to prepare a premix liquid; adding Al2O3 powder, B4C powder and the premix liquid in a ball milling tank to be ball-milled and dispersed to prepare a slurry with solid phase content of not less than 50vol percent and viscosity of not more than 1Pa.s; adding ammonium persulfate and tetramethyl ethylene diamine in the slurry, and uniformly mixing; and pouring the uniformly mixed slurry into a die, completely solidifying the slurry, and removing the die to obtain a green Al2O3-B4C material. The prepared green Al2O3-B4C material has uniform density, organic matter content less than 5wt% and bending strength more than 15MPa, can undergo machining, accurately controls the size, and reduces the machining allowance of a sintering body to be minimum.

Description

Al 2O 3-B 4The notes of the C material type method of congealing into

Technical field

The invention belongs to nuclear fuel and material preparation method, be specifically related to a kind of Al that is used for the nuclear power station presurized water reactor ₂O ₃-B ₄The preparation method of C burnable poison stupalith.

Background technology

Al ₂O ₃-B ₄The many forms with sintered ceramic components of C are used in and make the neutron absorbing material in the presurized water reactor, its objective is to flatten initial loading stockpile core distribute power, prolong the phase in fuel longevity.Adopt dry method powder batch mixing, mold pressing or heat pressing process to prepare Al both at home and abroad ₂O ₃-B ₄The C ceramic component is like the disclosed " Al of 1993 the 5th phases " Nuclear Power Engineering " 437-439 page or leaf ₂O ₃-B ₄The development of C disperse ceramic pellet ", the 18th phase of nineteen eighty-three " the Journal of Materials Science " disclosed " SinteringAl of 669-677 page or leaf ₂O ₃-B ₄C Ceramics ", adopt mold pressing or heat pressing process to produce Al ₂O ₃-B ₄C disperse ceramic component, its defective is: adopt mold pressing or heat pressing process to produce Al ₂O ₃-B ₄C disperse ceramic component, mould take high, and production efficiency is low, and process redundancy is big behind the product, and dimensional accuracy can not guarantee.

Summary of the invention

The objective of the invention is to: a kind of Al is provided ₂O ₃-B ₄The notes of the C material type method of congealing into, this method can overcome Al ₂O ₃-B ₄It is high to adopt mold pressing or heat pressing process to have the mould expense in the C material preparation, and production efficiency is low, and process redundancy is big behind the product, and dimensional accuracy such as can not guarantee at shortcoming.

Technical scheme of the present invention is following:

A kind of Al ₂O ₃-B ₄The notes of the C material type method of congealing into, step is:

The first step; With organic monomer N hydroxymethyl acrylamide, crosslinking chemical subunit bisacrylamide and spreading agent ammonium polyacrylate and the mixed premixed liquid of preparing of deionized water; Wherein the deionized water consumption is 100ml, and said organic monomer and dosage of crosslinking agent are 20～50: 1 with the weight ratio of gram metering; The consumption of spreading agent ammonium polyacrylate is 3～8 grams;

Step 2 adds Al in ball grinder ₂O ₃Powder, B ₄C powder and abrading-ball add the premixed liquid of preparation wherein, and Ball milling 2～6 hours is prepared the slurry of solid load>=50vol%, viscosity≤1Pas;

Step 3 adds the initiator ammonium persulfate of 0.5～2ml in the slurry, and the catalyzer tetramethylethylenediamine of 0.2～1ml mixes;

Step 4 in mould, left standstill the slurry perfusion that mixes 30 minutes under the room temperature, slurry solidifies fully, sloughs mould, obtains Al ₂O ₃-B ₄C material green compact.

Additional technical feature is: used Al in the step 2 ₂O ₃Powder and B ₄The part by weight of C powder is 10～50: 1.

Effect of the present invention is: according to the Al of the inventive method preparation ₂O ₃-B ₄C material green compact, it is even to have a blank density, and relative density reaches 55%～65%; Organic content＜5wt%, bending strength＞15MPa, B ₄Advantages such as C is evenly distributed, first base can stand machining, and size is accurately controlled, and drops to the process redundancy of sintered body minimum.

Embodiment

Embodiment 1

1. in the 100ml deionized water, add N hydroxymethyl acrylamide 10g, subunit bisacrylamide 0.5g, ammonium polyacrylate 3g prepares premixed liquid; Wherein: the weight ratio of N hydroxymethyl acrylamide and subunit bisacrylamide is 20: 1;

2. in ball grinder, add 500gAl ₂O ₃Ball, 500gAl ₂O ₃Powder, 50g B ₄The C powder adds the premixed liquid of preparing wherein, and ball milling 2 hours is with slurry and Al ₂O ₃Ball separates, and prepares Al ₂O ₃-B ₄The C slip; Wherein: Al ₂O ₃Powder and B ₄The weight ratio of C powder is 10: 1;

3. at Al ₂O ₃-B ₄The C slip adds ammonium persulfate 0.5ml, tetramethylethylenediamine 0.2ml, mixes;

4. the slip that mixes is filled in the mould, left standstill under the room temperature 30 minutes, slip solidifies fully, sloughs mould, obtains Al ₂O ₃-B ₄C material green compact.

Embodiment 2

1. in the 100ml deionized water, add N hydroxymethyl acrylamide 10g, subunit bisacrylamide 0.33g, ammonium polyacrylate 5g prepares premixed liquid; Wherein: the weight ratio of N hydroxymethyl acrylamide and subunit bisacrylamide is 30.3: 1;

2. in ball grinder, add 500gAl ₂O ₃Ball, 300gAl ₂O ₃Powder, 10g B ₄The C powder adds the premixed liquid of preparing wherein, and ball milling 4 hours is with slurry and Al ₂O ₃Ball separates, and prepares Al ₂O ₃-B ₄The C slip; Wherein: Al ₂O ₃Powder and B ₄The weight ratio of C powder is 30: 1;

3. at Al ₂O ₃-B ₄The C slip adds ammonium persulfate 1.0ml, tetramethylethylenediamine 0.5ml, mixes;

4. the slip that mixes is filled in the mould, left standstill under the room temperature 30 minutes, slip solidifies fully, sloughs mould, obtains Al ₂O ₃-B ₄C material green compact.

Embodiment 3

1. in the 100ml deionized water, add N hydroxymethyl acrylamide 10g, subunit bisacrylamide 0.2g, ammonium polyacrylate 8g prepares premixed liquid; Wherein: the weight ratio of N hydroxymethyl acrylamide and subunit bisacrylamide is 50: 1;

2. in ball grinder, add 500gAl ₂O ₃Ball, 400g Al ₂O ₃Powder, 8g B ₄The C powder adds the premixed liquid of preparing wherein, and ball milling 6 hours is with slurry and Al ₂O ₃Ball separates, and prepares Al ₂O ₃-B ₄The C slip; Al wherein ₂O ₃Powder and B ₄The weight ratio of C powder is 50: 1;

3. at Al ₂O ₃-B ₄The C slip adds ammonium persulfate 2ml, tetramethylethylenediamine 1ml, mixes;

4. with the Al that mixes ₂O ₃-B ₄The C slip is filled in the mould, leaves standstill under the room temperature 30 minutes, and slip solidifies fully, sloughs mould, obtains Al ₂O ₃-B ₄C material green compact.

Claims (2)

1. Al ₂O ₃-B ₄The notes of the C material type method of congealing into, step is:

The first step; With organic monomer N hydroxymethyl acrylamide, crosslinking chemical subunit bisacrylamide and spreading agent ammonium polyacrylate and the mixed premixed liquid of preparing of deionized water; Wherein the deionized water consumption is 100ml, said organic monomer and dosage of crosslinking agent, and the weight ratio of measuring with gram is 20～50: 1; The consumption of spreading agent ammonium polyacrylate is 3～8 grams;

Step 2 adds Al in ball grinder ₂O ₃Powder, B ₄C powder and abrading-ball add the premixed liquid of preparation wherein, and Ball milling 2～6 hours is prepared the slurry of solid load>=50vol%, viscosity≤1Pas;

Step 3 adds the initiator ammonium persulfate of 0.5～2ml in the slurry, and the catalyzer tetramethylethylenediamine of 0.2～1ml mixes;

Step 4 in mould, left standstill the slurry perfusion that mixes 30 minutes under the room temperature, slurry solidifies fully, sloughs mould, obtains Al ₂O ₃-B ₄C material green compact.

2. according to the described Al of claim 1 ₂O ₃-B ₄The notes of the C material type method of congealing into is characterized in that: used Al in the step 2 ₂O ₃Powder and B ₄The weight ratio of C powder is 10～50: 1.